CN102183501A - Quick detection method for resonance light scattering of perfluorooctane sulfonate (PFOS) in environmental water sample - Google Patents
Quick detection method for resonance light scattering of perfluorooctane sulfonate (PFOS) in environmental water sample Download PDFInfo
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- CN102183501A CN102183501A CN 201110065276 CN201110065276A CN102183501A CN 102183501 A CN102183501 A CN 102183501A CN 201110065276 CN201110065276 CN 201110065276 CN 201110065276 A CN201110065276 A CN 201110065276A CN 102183501 A CN102183501 A CN 102183501A
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Abstract
The invention discloses a quick detection method for resonance light scattering of perfluorooctane sulfonate (PFOS) in an environmental water sample, and relates to the field of environmental analysis. A resonance light scattering analysis method is adopted in the method. The method comprises the following steps of: sequentially adding 0.40mL of 4.2*10<-4>mol/L rhodamine 6G solution and 1.0mL of butadiene rubber (BR) buffer solution with pH of 3.29 into a 10mL color comparison tube, swirling the solution uniformly, and adding the pretreated water sample to be detected; after uniform swirling mixing, fixing the volume to 10mL by using 18.2Momega ultrapure water, and immediately performing synchronous scanning on a fluorescence spectrophotometer in lambda ex=lambda em, wherein both the excitation slit and the emission slit are 5 nanometers, and the voltage is 400V; recording the scattered spectrum in a wavelength range of 220 to 420 nanometers; and performing preliminary qualitative analysis and quantitative analysis on whether the environmental water sample contains the PFOS according to the scattered signals at the wavelength of 313 nanometers. If the water sample contains the PFOS, the scattering intensity at the wavelength of 313 nanometers is enhanced; otherwise, the scattered signals at the wavelength of 313 nanometers are not changed. The invention is characterized in that: the method for detecting the PFOS in the environmental water sample is simple, quick and sensitive, and low in detection cost.
Description
Technical field
The present invention relates to the detection method of PFOS in the environmental analysis field, particularly environmental water sample.
Background technology
Perfluorooctane sulfonates (Perfluorooctane sulfonate, PFOS) be representative substances in the numerous perfluorochemical family, be widely used in industry and civilian industries such as weaving, papermaking, packing, agricultural chemicals, carpet, leather, floor polishing, plating, fire foam and shampoo.The perfluor series compound that contains PFOS in vivo or the kalabolism end-product in the environment be PFOS.PFOS has good thermal stability and chemical inertness, can tolerate Guang Zhao ﹑ Gao Wen ﹑ization ﹑ microorganism and high vertebrate metabolism and be difficult to the degraded.Studies show that also do not decompose even PFOS boils 1h in concentrated nitric acid solution, hydrolysising half-life was greater than 41 years, the photodissociation half life period was greater than 3.7 years.PFOS has the biological accumulation of height, and the PFOS in the water shifts to comprising that a human high position is biological by long-pending effect of hydrobiological richness and food chain approach.A large amount of investigation is found, PFOS has hereditary Du ﹑ arrenotoky Du ﹑ and grows Du ﹑ Shen through multiple toxicity such as Du ﹑ interference Jia shape gland Gong Neng ﹑ hepatotoxicity and endocrine interference effects, is considered to the pollutant that a class has many devices of whole body dysentery.
The PFOS problem of environmental pollution has caused the attention of related organization.U.S. environment administration, Canada, European Union etc. to PFOS use and standard has been carried out in production.2003,3M company of maximum in the world perfluorinated compound manufacturing enterprise stopped to produce Related product.On October 24th, 2006, parliament of European Union formally passes a resolution, and stipulates that the content of PFOS must not be above 0.005% of product quality in the manufactured goods on the European Union market.The U.S. has stipulated Ming Su Dazhou City that the maximum acceptable concentration (MPC) of PFOS is 0.3 in the potable water
G/L.In May, 2009, in the 4th conference of pact contracting party of holding in Geneva, perfluoro octyl sulfonic acid and salt thereof and full-fluorine octyl sulfuryl fluoride are formally listed in persistence organic pollutant list accessories B and are limited.Harm to environment and human body is also faced by scientist day by day, and the various countries scholar has carried out PFOS and studies in great detail.
At present, be used for the PFOS analysis and mainly contain using high performance liquid chromatography tandem mass spectrum (HPLC/MS/MS), high performance liquid chromatography mass spectrometry (HPLC/MS), gas chromatography mass spectrometry (GC/MS) isochromatic spectrum analytical approach.These methods all because of the instrument costliness, be unfavorable for popularizing.
Summary of the invention
The object of the invention is to invent that a kind of cost is low, simple, the method for PFOS in the fast detecting environmental water sample.
The present invention adopts resonance scattering method, and adding 0.40 mL concentration in 10 mL color comparison tubes successively is 4.2 * 10
-4The rhodamine 6G of mol/L (Rh6G) solution (catechol rhodamine 6G English name: Rhodamine 6G), the BR damping fluid of 1.0 mL pH 3.29, vortex is even, adds through pretreated water sample to be measured again; Use 18.2 M behind the whirlpool mixing
Ultrapure water is settled to 10 mL, behind the whirlpool mixing, on fluorospectrophotometer with
Carry out synchronous scanning, excite slit and emission slit to be 5 nm, voltage is 400 V, the scattering spectrum of record 220～420 nm scopes.Scattered signal according to 313 nm places carries out preliminary qualitative analysis and quantitative test to whether containing PFOS in the environmental water sample.
As containing PFOS in the tested water sample, then itself and rhodamine 6G can form ionic associate, cause 313 nm places scattered signals to strengthen.Adopt resonance scattering method, strengthen, then contain PFOS in the water sample,, then do not contain PFOS in the water sample as not strengthening as scattering spectrum 313 nm place scattered signals.This method detects and is limited to 9.95 nmol/L, and application of sample is finished and can be detected.
The invention has the advantages that:
1, this analytical approach is simple, only is rhodamine 6G-PFOS binary system.
2, this method is quick, can detect immediately after application of sample is finished.
3, this method detection cost is low, and required instrument only is common fluorospectrophotometer.
4, highly sensitive, can reach ng/mL, in conjunction with the separation and concentration of PFOS, detectability can be low to moderate ng/L.
In a word, the PFOS that this method is used for environmental water sample detects, have simple, quick, the low characteristics of detection cost, help actual promotion and application, can satisfy the actual needs that environmental water sample is analyzed, to using and discharging, environmental ecology damage and health effect of China assessment PFOS, and provide foundation to formulating Control Countermeasure, detoxifcation scheme and relevant laws and regulations.Also, PFOS in government department's supervision environment provides the analytical technology support simultaneously for polluting.
Description of drawings
Fig. 1 is the interactional resonant light scattering spectrogram of rhodamine 6G and PFOS.
1.?PFOS?2.?Rh6G;?3-6.?PFOS-Rh6G;?
c Rh6G:?16.0?μmol/L;?
c PFOS(μmol/L):?1,?10.0;?3,?5.0;?4,?10.0;?5,?15;?6,?20.?pH?3.29。
Embodiment
One, qualitative detection
Detection method: resonance scattering method.
Instrument: F-2500 type fluorospectrophotometer (HIT) is used for writing down and mensuration resonant light scattering spectrum and intensity.
Reagent: PFOS standard substance (purity is greater than 98.0%, and ladder is uncommon likes that (Shanghai) changes into industrial development company limited); Rhodamine 6G.
Working solution: directly use ultrapure water (18.2 M
) preparation 1.0 * 10
-4The PFOS solution and 4.2 * 10 of mol/L
-4Mol/L rhodamine 6G solution.With the acidity of the BR buffer solution hierarchy of control, it is pure that reagent is analysis, and experimental water is ultrapure water (18.2 M
).
Method of operating, initial analysis:
Resonance scattering method.
Adding 0.40 mL concentration in 10 mL color comparison tubes successively is 4.2 * 10
-4The rhodamine 6G solution of mol/L, the BR damping fluid of 1.0 mL pH 3.29, vortex is even, adds through pretreated water sample to be measured again; Use 18.2 M behind the whirlpool mixing
Ultrapure water is settled to 10 mL, behind the whirlpool mixing, immediately on fluorospectrophotometer with
Carry out synchronous scanning, excite slit and emission slit to be 5 nm, voltage is 400 V, the scattering spectrum of record 220～420 nm scopes.Whether the scattered signal of observing 313 nm places strengthens.
The result:
If 313 nm place scattered signals strengthen, shown among Fig. 13,4,5,6, show and contain PFOS in the water sample.
If do not strengthen, show in detectability, not contain PFOS in the water sample.
Two, quantitative test
Detection method: resonance scattering method.
Instrument: F-2500 type fluorospectrophotometer (HIT) is used for writing down and mensuration resonant light scattering spectrum and intensity.
Reagent: PFOS standard substance (purity is greater than 98.0%, and ladder is uncommon likes that (Shanghai) changes into industrial development company limited); Rhodamine 6G.
Working solution: directly use ultrapure water (18.2 M
) preparation 1.0 * 10
-4The PFOS solution and 4.2 * 10 of mol/L
-4Mol/L rhodamine 6G solution.With the acidity of the BR buffer solution hierarchy of control, it is pure that reagent is analysis, and experimental water is ultrapure water (18.2 M
).
Method of operating, initial analysis:
Resonance scattering method.
Adding 0.40 mL concentration in 10 mL color comparison tubes successively is 4.2 * 10
-4The rhodamine 6G solution of mol/L, the BR damping fluid of 1.0 mL pH 3.29, vortex is even, adds the PFOS of variable concentrations again; Use 18.2M behind the whirlpool mixing
Ultrapure water is settled to 10 mL, behind the whirlpool mixing, on fluorospectrophotometer with
Carry out synchronous scanning, excite slit and emission slit to be 5 nm, voltage is 400 V, the scattering spectrum of record 220～420 nm scopes.D with 313 nm places
I RLSTo the mapping of corresponding PFOS concentration, the drawing standard curve, and with the content of PFOS in the standard addition method detection by quantitative environmental water sample.
The result: the scattered signal at 313 nm places is directly proportional with the concentration of PFOS, as shown in Figure 1, and with the content of PFOS in the standard addition method detection by quantitative environmental water sample.
Three, the pre-service of water sample to be measured
Because PFOS content is relatively low in the environmental water sample, need carry out the separation and concentration pre-service usually.Water sample pre-service to be measured uses existing P FOS method for separating and concentrating to carry out, as solid-phase microextraction-high performance liquid chromatography isolation technics, sample collecting is after membrane filtration removes the middle suspension that anhydrates, use the solid-phase microextraction column extracting, use methanol-eluted fractions, the back concentrates with the high pure nitrogen volatilization, through the further separating treatment of HPLC.
Claims (2)
1. the resonant light scattering method for quick of PFOS in the environmental water sample is characterized in that adopting resonance scattering method, and adding 0.40 mL concentration in 10 mL color comparison tubes successively is 4.2 * 10
-4The rhodamine 6G solution of mol/L, the BR damping fluid of 1.0 mL pH 3.29, vortex is even, adds through pretreated water sample to be measured again; Be settled to 10 mL with 18.2 M Ω ultrapure waters behind the whirlpool mixing, behind the whirlpool mixing, immediately on fluorospectrophotometer with
Carry out synchronous scanning, excite slit and emission slit to be 5 nm, voltage is 400 V, the scattering spectrum of record 220～420 nm scopes; Scattered signal according to 313 nm places carries out preliminary qualitative analysis to whether containing PFOS in the environmental water sample, as detects scattering spectrum 313 nm places scattered signals enhancing, then contains PFOS in the water sample, as not strengthening, does not then contain PFOS in the water sample.
2. the resonant light scattering method for quick of PFOS in the environmental water sample according to claim 1, it is characterized in that further carrying out quantitative test to containing PFOS in the environmental water sample: adding 0.40 mL concentration in 10 mL color comparison tubes successively is 4.2 * 10
-4The rhodamine 6G solution of mol/L, the BR damping fluid of 1.0 mL pH 3.29, vortex is even, adds the PFOS standard substance of variable concentrations again; Be settled to 10 mL with 18.2M Ω ultrapure water behind the whirlpool mixing, behind the whirlpool mixing, immediately on fluorospectrophotometer with
Carry out synchronous scanning, excite slit and emission slit to be 5 nm, voltage is 400 V, the scattering spectrum of record 220～420 nm scopes, with 313 nm places
I RLSTo the mapping of corresponding PFOS concentration, the drawing standard curve, and with the content of PFOS in the standard addition method detection by quantitative environmental water sample.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507514A (en) * | 2011-09-30 | 2012-06-20 | 西南大学 | Determination method for light scattering/fluorescence ratio of PFOS (Perfluorooctane Sulfonates) in environment water sample |
| CN102645422A (en) * | 2012-04-13 | 2012-08-22 | 广西师范大学 | Method for measuring pipemidic acid by using resonance scattering spectrum |
| CN103558198A (en) * | 2013-07-22 | 2014-02-05 | 西南大学 | Fluorescent rapid detection method for PFOS (Perfluorooctane Sulfonates) in environmental water sample |
| CN106706588A (en) * | 2017-01-16 | 2017-05-24 | 南华大学 | Heterogeneous photocatalysis resonance fluorescence method for accurately detecting trace uranium in environmental water sample |
| CN110749574A (en) * | 2019-11-05 | 2020-02-04 | 广东药科大学 | Method for measuring perfluorooctane sulfonate by dual-wavelength resonance Rayleigh scattering method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101576490A (en) * | 2009-06-12 | 2009-11-11 | 广西师范大学 | Catalytic reaction-resonance scattering spectroscopic method for detecting trace molybdenum |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101576490A (en) * | 2009-06-12 | 2009-11-11 | 广西师范大学 | Catalytic reaction-resonance scattering spectroscopic method for detecting trace molybdenum |
Non-Patent Citations (2)
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| 《分析测试学报》 20040331 贺冬秀等 共振光散射法测定环境水样中痕量铬(VI) 89-91 1-2 第23卷, 第2期 * |
| 《淮北煤炭师范学院学报（自然科学版）》 20071231 董存智 罗丹明6G共振光散射法测定痕量亚硝酸根 35-37 1-2 第28卷, 第4期 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507514A (en) * | 2011-09-30 | 2012-06-20 | 西南大学 | Determination method for light scattering/fluorescence ratio of PFOS (Perfluorooctane Sulfonates) in environment water sample |
| CN102645422A (en) * | 2012-04-13 | 2012-08-22 | 广西师范大学 | Method for measuring pipemidic acid by using resonance scattering spectrum |
| CN102645422B (en) * | 2012-04-13 | 2014-04-16 | 广西师范大学 | Method for measuring pipemidic acid by using resonance scattering spectrum |
| CN103558198A (en) * | 2013-07-22 | 2014-02-05 | 西南大学 | Fluorescent rapid detection method for PFOS (Perfluorooctane Sulfonates) in environmental water sample |
| CN103558198B (en) * | 2013-07-22 | 2016-03-23 | 西南大学 | The fluorescence method for quick of PFOS in environmental water sample |
| CN106706588A (en) * | 2017-01-16 | 2017-05-24 | 南华大学 | Heterogeneous photocatalysis resonance fluorescence method for accurately detecting trace uranium in environmental water sample |
| CN106706588B (en) * | 2017-01-16 | 2019-08-16 | 南华大学 | A kind of accurate multiphase photocatalysis resonance fluorescence method for detecting determination of trace uranium in environmental water sample |
| CN110749574A (en) * | 2019-11-05 | 2020-02-04 | 广东药科大学 | Method for measuring perfluorooctane sulfonate by dual-wavelength resonance Rayleigh scattering method and application |
| CN110749574B (en) * | 2019-11-05 | 2021-11-02 | 广东药科大学 | Method for measuring perfluorooctane sulfonate by dual-wavelength resonance Rayleigh scattering method and application |
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